Plugging problems observed in severe hydrocracking of vacuum residue

Carbons deposited on the filter after the reactor of hydrocracking (US-Sludge) and in the heat exchanger (DS-Sludge) in a commercial H-Oil process were analyzed through the elemental analysis, XRD, SEM, optical microscope, 13C-NMR and Raman spectroscopy to elucidate their formation mechanism. Heat treatment of sludge and oil products recovered from the commercial process was performed at 698 K of a reaction temperature. XRD showed the presence of Fe1−xS, NaCl, and CaSO4 as well as carbon (2Θ = 26.6°) in US-Sludge. The carbon showed medium and fine mosaic textures surrounding the isotropic grains. DS-Sludge showed mixed texture of domain and flow surrounding the fine mosaic grains. The sludge consisted of stacked carbon flakes with a number of pores on the surface. EDX showed dominant presence of NaCl and CaO particles in the mosaic region. Heat treatment of asphaltene in the product mixed with US-Sludge gave the same appearance to that of DS-Sludge. US- and DS-Sludge are concluded to be formed through the respective carbon formation in the reactor and to be separated on the filter and on the heat exchanger surface, respectively. The carbon particles produced in the reactor collect contaminant Fe1−xS and CaSO4 particles to form the agglomerate where the growth and coalescence of the anisotropic spheres are very restricted to form the fine mosaic texture as observed in the US-Sludge. In contrast, the carbonization of the major precipitated heavy aromatic component leads to the domain or flow anisotropic texture through rather free growth and coalescence of anisotropic spheres on the surface of the heat exchanger wall. Although some parts of precipitated component together with US-Sludge give mosaic texture through the restricted growth and coalescence of anisotropic sphere by the presence of reactive fine solids.